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ChemicalBook CAS DataBase List Methyl 2,5-bis(2,2,2-trifluoroethoxy)benzoate
175204-89-4

Methyl 2,5-bis(2,2,2-trifluoroethoxy)benzoate synthesis

2synthesis methods
-

Yield:175204-89-4 100%

Reaction Conditions:

with sulfuric acid at 120; for 1 h;Microwave irradiation;

Steps:

1 Methyl 2-hydroxy-5-(trifluoromethoxy)benzoate (AED011-095)

A mixture of 2 -hydroxy-5 - (trifluoromethoxy)benzoic acid (300 mg, 1.35 mmol) and a few drops of concentrated H2SO4 was heated to 120 °C for 1 h under microwave irradiation, after which LC-MS analysis showed completion. Reaction mixture was concentrated to dryness to afford methyl 2 -hydroxy-5 -(trifluoromethoxy)benzoate (319 mg, 100 % yield) as a white solid, which was used without further purification. NMR (400 MHz, DMSO-ck) d 10.57 (s, 1H), 7.65 (d, J= 3.2 Hz, 1H), 7.54 (dt, J= 9.4, 3.0 Hz, 1H), 7.10 (d, J= 9.1 Hz, 1H), 3.89 (s, 3H). 19F NMR (376 MHz, DMSO-ifc) d -57.17 (s, 3F). LCMS RT (Method 2) = 3.507 min.

References:

WO2019/173761,2019,A1 Location in patent:Page/Page column 95

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